U.S. patent application number 12/408913 was filed with the patent office on 2010-01-28 for reduction of free radicals in crosslinked polyethylene by infrared heating.
This patent application is currently assigned to ZIMMER, INC.. Invention is credited to Hallie E. Brinkerhuff, Michael E. Hawkins, Dirk Pletcher, Alicia Rufner, Brian H. Thomas, Donald Yakimicki.
Application Number | 20100022678 12/408913 |
Document ID | / |
Family ID | 41569217 |
Filed Date | 2010-01-28 |
United States Patent
Application |
20100022678 |
Kind Code |
A1 |
Yakimicki; Donald ; et
al. |
January 28, 2010 |
REDUCTION OF FREE RADICALS IN CROSSLINKED POLYETHYLENE BY INFRARED
HEATING
Abstract
UHMWPE is exposed to crosslinking radiation and than heated
utilizing infrared radiation in an inert environment. In one
exemplary embodiment, the infrared radiation is provided by an
infrared heater having a tungsten heating element with a quartz
tube. In this embodiment, the infrared radiation may have the
wavelength from about 1.0 micron to about 1.5 microns. In another
exemplary embodiment, the UHMWPE is compression molded into bars
prior to exposure to the crosslinking radiation.
Inventors: |
Yakimicki; Donald; (Warsaw,
IN) ; Thomas; Brian H.; (Columbia City, IN) ;
Rufner; Alicia; (Columbia City, IN) ; Pletcher;
Dirk; (Walkerton, IN) ; Brinkerhuff; Hallie E.;
(Winona Lake, IN) ; Hawkins; Michael E.; (Columbia
City, IN) |
Correspondence
Address: |
ZIMMER TECHNOLOGY - BAKER & DANIELS
111 EAST WAYNE STREET, SUITE 800
FORT WAYNE
IN
46802
US
|
Assignee: |
ZIMMER, INC.
Warsaw
IN
|
Family ID: |
41569217 |
Appl. No.: |
12/408913 |
Filed: |
March 23, 2009 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
12179170 |
Jul 24, 2008 |
|
|
|
12408913 |
|
|
|
|
Current U.S.
Class: |
522/161 ;
525/333.7 |
Current CPC
Class: |
B29C 71/02 20130101;
B29C 71/04 20130101; C08J 7/08 20130101; C08J 3/28 20130101; B29C
2035/0822 20130101; B29K 2023/0683 20130101; B29C 2791/005
20130101; A61L 27/16 20130101; B29L 2031/7532 20130101; C08J 3/247
20130101; C08L 23/06 20130101; A61L 27/16 20130101; B29C 2071/022
20130101; C08J 2323/06 20130101 |
Class at
Publication: |
522/161 ;
525/333.7 |
International
Class: |
C08F 10/02 20060101
C08F010/02; C08J 3/28 20060101 C08J003/28 |
Claims
1. A method of processing UHMWPE for medical device applications,
the method comprising the steps of: providing a quantity of UHMWPE;
crosslinking the UHMWPE; and heating the UHMWPE by exposing the
UHMWPE to thermal radiation in an inert environment at a watt
density of at least 1 watt per square centimeter.
2. The method of claim 1, further comprising, before the heating
step, the steps of positioning the UHMWPE in a container and
creating an inert environment in the container.
3. The method of claim 2, wherein the container is formed from
glass.
4. The method of claim 2, wherein the container is formed from
nylon.
5. The method of claim 1, wherein the thermal radiation comprises
infrared radiation.
6. The method of claim 1, wherein the heating step further
comprises heating the UHMWPE above a melting point of the UHMWPE to
melt anneal the UHMWPE, wherein the melting point is determined by
differential scanning calorimetry.
7. The method of claim 1, wherein the heating step further
comprises heating the UHMWPE above 140 degrees Celsius.
8. The method of claim 1, wherein the infrared radiation comprises
a wavelength of substantially between 1.0 microns and 15
microns.
9. The method of claim 8, wherein the infrared radiation comprises
a wavelength of substantially between 1.0 microns and 1.5
microns.
10. The method of claim 1, wherein the crosslinking step further
comprises exposing the UHMWPE to crosslinking irradiation.
11. The method of claim 10, wherein the crosslinking step further
comprises exposing the UHMWPE to electron beam irradiation.
12. The method of claim 1, further comprising the step of
compression molding the UHMWPE.
13. The method of claim 1, further comprising, before the
crosslinking step, the step of preheating the UHMWPE.
14. The method of claim 13, wherein the preheating step further
comprises preheating the UHMWPE using infrared radiation.
15. The method of claim 1, further comprising the step of machining
the UHMWPE to form a medical device.
16. A crosslinked UHMWPE for use in medical implants prepared by a
process comprising the steps of: providing a quantity of UHMWPE;
crosslinking the UHMWPE; and heating the UHMWPE by exposing the
UHMWPE to thermal radiation in an inert environment at a watt
density of at least 1 watt per square centimeter.
17. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has an
ultimate tensile strength of at least 32 megapascal.
18. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has an
izod impact strength of at least 55 kilojoules per square
meter.
19. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has a
yield strength of at least 20 megapascals.
20. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has an
electron spin resonance below 0.10.times.10.sup.15 spins per
gram.
21. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has an
ultimate tensile strength of at least 32 megapascal, an izod impact
strength of at least 55 kilojoules per square meter, and an
elongation of at least 200 percent.
22. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has a
yield strength of at least 20 megapascals, a storage modulus of at
least 6.0 megapascals at two hundred degrees Celsius, and an
electron spin resonance below 0.10.times.10.sup.15 spins per
gram.
23. The crosslinked UHMWPE of claim 16, wherein the UHMWPE has an
oxidative index at an exterior surface of the UHMWPE of less than
0.1000.
Description
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation-in-part of co-pending
U.S. patent application Ser. No. 12/179,170, entitled "REDUCTION OF
FREE RADICALS IN CROSSLINKED POLYETHYLENE BY INFRARED HEATING",
filed on Jul. 24, 2008, the entire disclosure of which is expressly
incorporated by reference herein.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The present invention relates to crosslinked ultra-high
molecular weight polyethylene and, particularly, to annealed,
crosslinked ultra-high molecular weight polyethylene.
[0004] 2. Description of the Related Art
[0005] Ultra-high molecular weight polyethylene (UHMWPE) is
commonly utilized in medical device applications. In order to
beneficially alter the material properties of UHMWPE and decrease
its wear rate, UHMWPE may be crosslinked. For example, UHMWPE may
be subjected to electron beam or gamma radiation, causing chain
scission of the individual polyethylene molecules as well as the
breaking of C--H bonds to form free radicals on the polymer chains.
While free radicals on adjacent polymer chains may bond to one
another to form crosslinked UHMWPE, some free radicals may remain
in the UHMWPE following irradiation, which could potentially
combine with oxygen and result in oxidation of the UHMWPE.
Oxidation may detrimentally affect the wear properties of the
UHMWPE and may also increase its wear rate. As a result, the
oxidized layer of the UHMWPE, which may be a significant depth of
the outer portion of the UHMWPE, may need to be removed prior to
utilizing the UHMWPE in medical device applications.
[0006] To help eliminate the free radicals that are formed during
irradiation that fail to cross-link and therefore may cause
oxidation, the UHMWPE may be melt annealed by heating the
crosslinked UHMWPE to a temperature in excess of its melting point.
By increasing the temperature of the UHMWPE above its melting
point, the mobility of the individual polyethylene molecules
significantly increases, facilitating additional crosslinking of
the polyethylene molecules and the quenching of free radicals. To
heat the UHMWPE above its melting point, the UHMWPE may be placed
in a convection oven in ambient air. A convection oven operates by
activating a heating element or burner that comes in contact with
the ambient air in the oven. By contacting the heating element or
burner, the internal energy of the air is increased, causing a
corresponding increase in its temperature. The air, in turn, then
contacts the UHMWPE and increases the internal energy of the
UHMWPE, causing a corresponding increase in the temperature of the
UHMWPE.
SUMMARY
[0007] The present invention relates to reducing the concentration
of free radicals in crosslinked UHMWPE. In one exemplary
embodiment, UHMWPE is exposed to crosslinking radiation and is then
heated by thermal radiation. For example, the use of thermal
radiation may replace the use of convection to heat the UHMWPE. In
convection heating, a heat source, such as a heating element or
open flame, is used to increase the temperature of an intermediate
medium, such as air or water, that then contacts the object to be
heated and transfers thermal energy thereto. As a result,
convection heating cannot work in a vacuum. In contrast, thermal
radiation does not require an intermediate medium as it utilizes
electromagnetic waves that are absorbed by the object to be heated.
The absorption of the electromagnetic waves by the object to be
heated results in an increase in the thermal energy of the object
and, correspondingly, an increase in the temperature of the
object.
[0008] In one exemplary embodiment, the UHMWPE is exposed to
infrared radiation. In this embodiment, the infrared radiation
generated may be in the near infrared spectrum, the mid infrared
spectrum, or the far infrared spectrum. In particular, the infrared
radiation generated may have a wavelength from approximately one
micron to fifteen microns. In one exemplary embodiment, the
infrared radiation is provided by an infrared heater having a
tungsten heating element with a quartz tube. In this embodiment,
the infrared radiation may have the wavelength from about 0.50
micron to about 5.0 microns. In another exemplary embodiment, the
UHMWPE is compression molded into bars prior to exposure to the
crosslinking radiation.
[0009] In one exemplary embodiment, once the UHMWPE bars are
crosslinked, the UHMWPE bars are hung from a rotating conveyor for
exposure to the infrared radiation. In another exemplary
embodiment, the UHMWPE bars are placed on a rack for exposure to
the infrared radiation. In yet another embodiment, the UHMWPE bars
may be placed on a conveyor that travels through an oven having a
plurality of infrared heating elements. As the bars travel through
the oven, the UHMWPE bars are exposed to the infrared radiation. In
order to decrease the heating of the air between the infrared
heating element and the UHMWPE bar, a fan may be used to move warm
air away from the UHMWPE bar and draw cooler air toward the UHMWPE
bar. By keeping the air surrounding the UHMWPE bar at a lower
temperature during irradiation, the surrounding air is less
reactive, lessening the likelihood of the UHMWPE bar experiencing
surface oxidation while annealing. In one exemplary embodiment, a
plurality of infrared heating elements and a plurality of fans are
arranged to facilitate the desired heating of the UHMWPE bar and
also to achieve the desired movement of air surrounding the UHMWPE
bar.
[0010] Alternatively, in another exemplary embodiment, the UHMWPE
bar may be exposed to thermal radiation in an inert environment.
For example, the UHMWPE bar may be placed within a container that
is flushed with an inert gas, such as nitrogen. In other exemplary
embodiments, the inert gas is a noble gas. Additionally, in order
to expose a plurality of UHMWPE bars to thermal radiation, such as
infrared radiation, in an inert environment, a plurality of
containers, each of the containers having an individual UHMWPE bar
positioned therein, may be connected to one another. In this
embodiment, an inert gas flows into one container and then travels
through each of the plurality of containers to force air out of the
containers sequentially. In this manner, an inert environment is
created in each of the containers.
[0011] In one exemplary embodiment, the containers for holding the
UHMWPE bars are formed from a material that allows shorter
wavelength infrared radiation to pass therethrough, while blocking
longer wavelength infrared radiation. In one exemplary embodiment,
the containers are made from glass. In another exemplary
embodiment, the containers are formed from nylon. In this
embodiment, the containers may be made from a flexible form of
nylon, such as nylon bags or, alternatively, may be formed as rigid
nylon structures. For example, in the embodiment in which a
container is formed from a nylon bag, the bag may be vacuum packed
to the UHMWPE bar to create an effective inert environment. In
another exemplary embodiment, the UHMWPE bars are placed in a
vacuum oven that has been modified for use with thermal radiation
emitters, such as infrared heaters.
[0012] Advantageously, by utilizing infrared radiation to melt
anneal UHMWPE, oxidation of the exterior surface of the UHMWPE bar
is substantially lessened. For example, during traditional melt
annealing in a convection oven in ambient air, up to eight
millimeters of the UHMWPE bar may be oxidized and, thus, rendered
unsuitable for use in medical device applications. In contrast, by
infrared melt annealing the UHMWPE bars, two millimeters or less of
the UHMWPE bar is oxidized. Advantageously, this results in a
substantial cost savings as less of the UHMWPE bar is rendered
unsuitable for use in its intended application. Additionally, by
infrared melt annealing a UHMWPE bar in an inert environment, the
resulting UHMWPE bar is able to withstand higher temperatures
before experiencing melting. Also, by creating an inert environment
and substantially eliminating any oxygen around the UHMWPE bar,
oxidation of the exterior surface of the UHMWPE bar is further
lessened.
[0013] Infrared melt annealing of the UHMWPE bar results in the
UHMWPE bar experiencing homogeneous heating and cooling, at a
substantially faster rate than in a convection oven. For example, a
conventional melt annealing cycle in a convection oven, which
begins with a temperature ramp up, extends through a temperature
hold, and ends with a temperature cool down, may be approximately
48 hours. In contrast, the use of infrared radiation to melt anneal
a UHMWPE bar may be performed in approximately eight hours or less.
This results in a substantial reduction in cycle time, which also
provides significant cost savings. Further, the need to utilize a
convection oven, which may be large, bulky, and expensive, is
obviated. A further decrease in the time needed to complete the
melt annealing cycle is achieved when the UHMWPE bars are infrared
melt annealed in an inert environment. This further decrease
results from the increased temperature of the inert gas that
surrounds the UHMWPE bar and provides an insulating effect.
[0014] In one form thereof, the present invention provides a method
of processing UHMWPE for medical device applications, the method
comprising the steps of: providing a quantity of UHMWPE;
crosslinking the UHMWPE; and heating the UHMWPE by exposing the
UHMWPE to thermal radiation in an inert environment at a watt
density of at least 1 watt per square centimeter.
[0015] In another form thereof, the present invention provides a
crosslinked UHMWPE for use in medical implants prepared by a
process comprising the steps of: providing a quantity of UHMWPE;
crosslinking the UHMWPE; and heating the UHMWPE by exposing the
UHMWPE to thermal radiation in an inert environment at a watt
density of at least 1 watt per square centimeter.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The above-mentioned and other features and advantages of
this invention, and the manner of attaining them, will become more
apparent and the invention itself will be better understood by
reference to the following descriptions of embodiments of the
invention taken in conjunction with the accompanying drawings,
wherein:
[0017] FIG. 1 is a perspective view of an exemplary device for
exposing an UHMWPE bar to infrared radiation;
[0018] FIG. 2 is a plan view of another exemplary device for
exposing an UHMWPE bar to infrared radiation;
[0019] FIG. 3 is a plan view of yet another exemplary device for
exposing an UHMWPE bar to infrared radiation;
[0020] FIG. 4 is a fragmentary, partial cross-sectional,
perspective view of the device of FIG. 3;
[0021] FIG. 5 is a partial cross-sectional view of an exemplary
mechanism for use in conjunction with the device of FIGS. 3 and
4;
[0022] FIG. 6 is a front elevational view of an UHMWPE bar in
conjunction with a device for retaining the UHMWPE bar in
position;
[0023] FIG. 7 is a cross-sectional view of the device of FIG. 6
taken along line 7-7 of FIG. 6;
[0024] FIG. 8 is a schematic view of an apparatus for exposing an
UHMWPE bar to infrared radiation according to another exemplary
embodiment;
[0025] FIG. 9 is an exploded perspective view of another exemplary
apparatus for retaining an UHMWPE bar in position;
[0026] FIG. 10 is a schematic view of another exemplary apparatus
for exposing a plurality of UHMWPE bars to infrared radiation;
[0027] FIG. 11 is a front elevational view of an exemplary conveyor
system for exposing UHMWPE bars to infrared radiation;
[0028] FIG. 12 is a cross-sectional view of the device of FIG. 11
taken along line 12-12 of FIG. 11;
[0029] FIG. 13 is a perspective view of an exemplary apparatus for
exposing an UHMWPE bar to infrared radiation;
[0030] FIG. 14 is a perspective view of another exemplary apparatus
for exposing an UHMWPE bar to infrared radiation;
[0031] FIG. 15 is an exploded, perspective view of an exemplary
embodiment of a device for exposing an UHMWPE bar to infrared
radiation in an inert environment;
[0032] FIG. 16 is a perspective view of the device of FIG. 15 in an
assembled state;
[0033] FIG. 17 is a perspective view of the device of FIG. 16
positioned between infrared heaters;
[0034] FIG. 18 is a plan view of a plurality of devices of FIG. 15
connected to one another;
[0035] FIG. 19 is a perspective view of another exemplary
embodiment of a device for exposing an UHMWPE bar to infrared
radiation;
[0036] FIG. 20 is a graphical depiction of the light transmittance
of Pyrex.RTM. 7740 borosilicate glass with transmittance percentage
on the y-axis and wavelength in nanometers on the x-axis;
[0037] FIG. 21 is a graphical depiction of the light transmittance
of nylon 6 or polycaprolactam with transmittance percentage on the
y-axis and wavelength in nanometers on the x-axis;
[0038] FIG. 22 is a graphical depiction of the normalized oxidative
index of an UHMWPE bar that was infrared melt annealed in an inert
atmosphere with the normalized oxidative index on the y-axis and
the depth from the surface of the bar in microns on the x-axis;
and
[0039] FIG. 23 is a graphical depiction of the normalized oxidative
index of an UHMWPE bar that was infrared melt annealed in air with
the normalized oxidative index on the y-axis and the depth from the
surface of the bar in microns on the x-axis.
[0040] Corresponding reference characters indicate corresponding
parts throughout the several views. The exemplifications set out
herein illustrate preferred embodiments of the invention and such
exemplifications are not to be construed as limiting the scope of
the invention in any manner.
DETAILED DESCRIPTION
[0041] In one exemplary embodiment of the present invention, UHMWPE
is exposed to crosslinking radiation and then melt annealed by
exposure to thermal radiation. In one exemplary embodiment, the
UHMWPE is melt annealed by exposure to infrared radiation. While
described herein with specific reference to infrared radiation, the
present invention may be used in conjunction with any type of
thermal radiation, such as microwave radiation or ultraviolet
radiation, for example.
[0042] Once annealed by exposure to infrared radiation, the UHMWPE
may be subjected to additional processing steps, such as packaging
and/or sterilization. Any medical grade UHMWPE powder may be
utilized in conjunction with the present invention to form a UHMWPE
bar or another form of stock material suitable for exposure to
crosslinking radiation. For example, GUR1050 and GUR1020 powders,
both commercially available from Ticona, having North American
headquarters located in Florence, Ky., may be used. In one
exemplary embodiment, the UHMWPE powder is blended with an
antioxidant. Exemplary methods for creating a UHMWPE/antioxidant
blend are disclosed in copending U.S. patent application Ser. No.
12/100,894, entitled AN ANTIOXIDANT STABILIZED CROSSLINKED
ULTRA-HIGH MOLECULAR WEIGHT POLYETHYLENE FOR MEDICAL DEVICE
APPLICATIONS, filed on Apr. 10, 2008, the entire disclosure of
which is expressly incorporated by reference herein. The UHMWPE
powder may then be processed by compression molding, net shape
molding, injection molding, ram extrusion, or monoblock formation,
for example.
[0043] In one exemplary embodiment, the UHMWPE is compression
molded into the form of a bar. In this embodiment, the UHMWPE bar
may be molded to a length of substantially between four feet and
five feet. Additionally, the UHMWPE bar may be molded into any
desired geometric shape, such that the UHMWPE bar has a
substantially round cross-section or a substantially square
cross-section, for example. Alternatively, the UHMWPE may be net
shape molded so that the UHMWPE has a shape substantially similar
to the shape of a final orthopedic component.
[0044] In another exemplary embodiment, the UHMWPE may be
compression molded into a substrate. In one exemplary embodiment,
the substrate may be a highly porous biomaterial useful as a bone
substitute and/or cell and tissue receptive material. A highly
porous biomaterial may have a porosity as low as 55, 65, or 75
percent or as high as 80, 85, or 90 percent. An example of such a
material is produced using Trabecular Metal.TM. technology
generally available from Zimmer, Inc., of Warsaw, Ind. Trabecular
Metal.TM. is a trademark of Zimmer Technology, Inc. Such a material
may be formed from a reticulated vitreous carbon foam substrate
which is infiltrated and coated with a biocompatible metal, such as
tantalum, etc., by a chemical vapor deposition ("CVD") process in
the manner disclosed in detail in U.S. Pat. No. 5,282,861, the
entire disclosure of which is expressly incorporated herein by
reference. In addition to tantalum, other metals such as niobium,
or alloys of tantalum and niobium with one another or with other
metals may also be used.
[0045] After processing, the UHMWPE may be heated to a temperature
below the melting point of the UHMWPE blend to relieve any residual
stresses that may have been formed during processing and to provide
additional dimensional stability. As used herein, the melting point
of the UHMWPE is the melting point as determined by ASTM
International F2625-07, Standard Test Method for Measurement of
Enthalpy of Fusion, Percent Crystallinity, and Melting Point of
Ultra-High-Molecular Weight Polyethylene by Means of Differential
Scanning Calorimetry. Heating the UHMWPE to a temperature below the
melting point of the UHMWPE creates a more homogenous mixture and
increases the final crystallinity. For example, the UHMWPE may be
preheated using a convection oven or by exposing the UHMWPE to
infrared radiation.
[0046] Irrespective of whether or not the UHMWPE is heated to a
temperature below the melting point of the UHMWPE to relieve any
residual stress, the processed UHMWPE may then by preheated in
preparation for receiving crosslinking irradiation. As used herein,
"crosslinking irradiation" refers to exposing the consolidated
UHMWPE blend to ionizing irradiation to form free radicals which
may later combine to form crosslinks. For example, the UHMWPE may
be preheated using a convection oven or by exposing the UHMWPE to
infrared radiation. In one exemplary embodiment, the processed
UHMWPE may be preheated to any temperature between room
temperature, approximately 23.degree. C., up to the melting point
of the UHMWPE, approximately 140.degree. C. In another exemplary
embodiment, the UHMWPE is preheated to a temperature between
60.degree. C and 130.degree. C. In other exemplary embodiments, the
UHMWPE may be heated to a temperature as low as 60.degree. C,
70.degree. C, 80.degree. C, 90.degree. C., or 100.degree. C. or as
high as 110.degree. C., 120.degree. C., 130.degree. C., 135.degree.
C., or 140.degree. C. By preheating the processed UHMWPE before
irradiation, the material properties of the resulting irradiated
UHMWPE are affected. Exemplary methods of preheating UHMWPE prior
to irradiation are disclosed in copending U.S. patent application
Ser. No. 12/100,894, which is expressly incorporated by reference
herein above. Thus, the material properties for a UHMWPE irradiated
at a relatively cold, e.g., approximately 40.degree. C.,
temperature are substantially different than the material
properties for a UHMWPE irradiated at a relatively warm, e.g.,
approximately 120.degree. C. to approximately 140.degree. C.,
temperature.
[0047] Once the UHMWPE is prepared as desired for crosslinking, the
UHMWPE may be exposed to crosslinking irradiation to induce
crosslinking of the UHMWPE. The irradiation may be performed in air
at atmospheric pressure, in a vacuum chamber at a pressure
substantially less then atmospheric pressure, or in an inert
environment, i.e., in an argon environment, for example. In one
exemplary embodiment, crosslinking is induced by exposing the
UHMWPE blend to a total radiation dose between about 25 kGy and
1,000 kGy. The irradiation is, in one exemplary embodiment,
electron beam irradiation. In another exemplary embodiment, the
irradiation is gamma irradiation. In yet another exemplary
embodiment, the crosslinking does not utilize radiation, but
instead utilizes silane or other forms of chemical
crosslinking.
[0048] Once the UHMWPE is irradiated, the UHMWPE may be heated
above its melting point, i.e., melt annealed, to decrease the free
radical concentration in the UHMWPE. In one exemplary embodiment,
the UHMWPE is heated above its melting point by exposing the UHMWPE
to infrared radiation. For example, the infrared radiation may be
provided to the UHMWPE at a watt density as low as 1.0, 1.5, 2.0,
2.5, 5.0, 10, or 20 watts per square centimeter and as high as 30,
40, 50, 60, 70, 80, or 100 watts per square centimeter. Exemplary
calculations of the watt density of an emitter are set forth in
Example 1 below.
[0049] Referring to FIG. 1, an exemplary apparatus 10 is shown for
exposing UHMWPE bar 12 to infrared radiation generated by infrared
heater 14. In one exemplary embodiment, infrared heater 14 utilizes
a tungsten filament positioned within a quartz tube to generate the
infrared radiation. While described herein with specific reference
to a tungsten filament positioned within a quartz tube, infrared
heater 14 may be utilized in conjunction with any filament and/or
tube capable of generating infrared radiation. Thus, infrared
heater 14 may generate infrared radiation in the near infrared
spectrum, the mid infrared spectrum, or the far infrared spectrum.
In one exemplary embodiment, infrared radiation having a wavelength
measured between adjacent crests of the wave from approximately one
micron to fifteen microns is generated. In the embodiment utilizing
a tungsten filament and quartz tube, the infrared radiation has a
wavelength of substantially between 1.0 microns and 1.5
microns.
[0050] Advantageously, infrared melt annealing of the UHMWPE bar
results in the UHMWPE bar experiencing homogeneous heating and
cooling at a substantially faster rate than in a convection oven.
For example, a conventional melt annealing cycle in a convection
oven may be approximately 48 hours. In contrast, the use of
infrared radiation to melt anneal a UHMWPE bar may be performed in
approximately three hours or less. Further, by utilizing infrared
radiation, the air or other medium that is surrounding the UHMWPE
bar remains at a lower temperature during annealing. As a result,
the surrounding air is less reactive, lessening the likelihood of
the UHMWPE bar experiencing surface oxidation during annealing.
[0051] Referring to FIG. 1, UHMWPE bar 12 is held in place by
rotatable plates 16, 18. Rotatable plate 16 is rotated by motor 20
causing corresponding rotation of UHMWPE bar 12 and plate 18, which
is freely rotatable about the longitudinal axis of UHMWPE bar 12.
At least partially surrounding UHMWPE bar 12 is reflective
shielding 22. By altering the amount of reflective shielding 22
surrounding UHMWPE bar 12, as well as the physical properties of
reflective shielding 22, the penetration and absorption of infrared
radiation by UHMWPE bar 12 may be altered. Fan 24 is positioned
below UHMWPE bar 12. Operation of fan 24 draws cool air from the
ambient environment and forces the same between UHMWPE bar 12 and
reflective shielding 22. This pushes the warmer air upward and out
from between the UHMWPE bar 12 and reflective shielding 22 through
opening 26 at the top of reflective shielding 22.
[0052] Operation of infrared heater 14 and fan 24 may be controlled
by temperature controller 28 having thermocouples 30, 32
electronically connected thereto. Thermocouples 30, 32 monitor the
temperature of the air surrounding UHMWPE bar 12 and the internal
temperature of UHMWPE bar 12, respectively. Based on the readings
from thermocouples 30, 32, controller 28 may turn infrared heater
14 on and off in order to reach and maintain a bar temperature in
excess of the melting point of the UHMWPE. Similarly, controller 28
may turn fan 24 on and off as needed to ensure that the air
temperature around UHMWPE bar 12 remains below a predetermined
temperature threshold. For example, in one exemplary embodiment,
controller 28 controls the operation of infrared heater 14 so that
the temperature of UHMWPE bar 12 is raised to and maintained at
substantially 150.degree. Celsius. However, controller 28 may be
configured to raise and maintain the temperature of UHMWPE bar 12
at any temperature in excess of the melting point of the UHMWPE.
Similarly, in one exemplary embodiment, controller 28 may activate
fan 24 when the temperature of the air around UHMWPE bar 12 exceeds
25.degree. Celsius. In another exemplary embodiment, controller 28
activates fan 24 to maintain the air temperature surrounding UHMWPE
bar 12 at substantially room temperature, e.g., 23.degree.
Celsius.
[0053] Referring to FIG. 2, another exemplary embodiment of an
apparatus for exposing UHMWPE bars to infrared radiation is
depicted as apparatus 40. As shown in FIG. 2, apparatus 40 includes
incoming UHMWPE bars 42 that have yet to be subjected to infrared
radiation and outgoing UHMWPE bars 44 that have already been
subjected to infrared radiation. Specifically, incoming UHMWPE bars
42 are received between opposing arms 46 of spindle 48, which is
rotating in a counter-clockwise direction. The counter-clockwise
rotation of spindle 48 may be achieved by the use of a motor, such
as motor 20 described above, mounted to spindle 48. As spindle 48
rotates, UHMWPE bars 42 are advance until they encounter an open
arm 50 of central spindle 52, which is also rotating in a
counter-clockwise direction. Similar to spindle 48, the rotation of
spindle 52 may be achieved by the use of a motor, such as motor 20
described above, mounted to spindle 52. Thus, as spindle 48
rotates, it advances incoming UHMWPE bar 42 toward an open arm 50
of central spindle 52 where connection portion 54 of an open arm 50
of central spindle 52 engages attachment member 56, as described in
detail below.
[0054] As central spindle 52 continues to rotate counter-clockwise
about centerpoint C, incoming UHMWPE bars 42 are exposed to
infrared radiation from infrared heaters 14, positioned at various
points throughout the path of central spindle 52. For example, in
one exemplary embodiment, infrared heaters 14 are positioned at
each corner 58, 60 defined by sections of outer reflective
shielding 62 and inner reflective shielding 64, respectively. In
another exemplary embodiment, panel heaters may be positioned
substantially entirely along portions of outer and inner reflective
shielding 62, 64. In one exemplary embodiment, fans 24, shown in
FIG. 1, may be positioned above and/or below apparatus 40 to
facilitate the transfer of air through apparatus 40 in a
substantially similar manner as described in detail above with
reference to apparatus 10. Additionally, as described in detail
above with specific reference to FIG. 1, a controller, such as
controller 28 (FIG. 1), may be used to control the operation of
infrared heaters 14 and, if used, fans 24. Additionally, the
controller may also be used to control the rate of rotation of
spindles 48, 52. Thus, by controlling the rate of rotation of
spindles 48, 52, the amount of time that it takes UHMWPE bars 42 to
travel through apparatus 40 may be adjusted.
[0055] As central spindle 52 continues to travel about centerpoint
C in a counter-clockwise direction, UHMWPE bars 42 may also be
rotated. For example, connection portions 54 of spindles 50 may
also be connected to a motor, such as motor 20 described above, by
a combination of shafts and/or gears to cause corresponding
rotation of UHMWPE bars 42. In one exemplary embodiment, connection
portions 54 are open on one side and rotate 180 degrees for every
45 degrees that center spindle 52 rotates. As a result, the open
end of connection portions 54 are aligned with attachment members
56 of UHMWPE bars 42 to allow connection portions 54 to engage
attachment members 56 of incoming UHMWPE bars 42 and disengage
attachment members 56 of outgoing UHMWPE bars 44. In this manner,
UHMWPE bars 42 eventually return to spindle 48 as outgoing UHMWPE
bars 44, i.e., UHMWPE bars that have been exposed to infrared
radiation, and are received between opposing arms 46 of spindle 48.
Specifically, outgoing UHMWPE bars 44 are retained between arms 46
of spindle 48 in a substantially similar manner as incoming UHMWPE
bars 42, described in detail above. As spindle 48 continues to
rotate, UHMWPE bars 44 are received by the track where they may be
transported to another location and/or apparatus for further
processing.
[0056] Referring to FIGS. 3-5, another exemplary apparatus for
exposing UHMWPE bars to infrared radiation is depicted as apparatus
80. Referring to FIG. 4, apparatus 80 includes conveyor 82 having a
plurality of connecting portions 54 configured for connecting to
attachment mechanisms 56 (FIG. 5), which are secured to UHMWPE bars
84. Additionally, in one exemplary embodiment, conveyor 80 may
further include rotation devices 96, described in detail below with
reference to FIG. 5, attached thereto. Apparatus 80 may further
include reflective shielding 86 positioned on inner and outer walls
85, 87, respectively, of apparatus 80. As UHMWPE bars 84 travel
through apparatus 80 along conveyor 82, they are exposed to
infrared radiation from a plurality of infrared heaters 14, shown
in FIG. 1. Infrared heaters 14 may be positioned within apparatus
80 in any configuration necessary to achieve the desired heating
affects in UHMWPE bars 84 and, as described in detail above with
reference to FIG. 1, may be controlled by controller 28. Apparatus
80 may further comprise fans 24, shown in FIG. 1, for regulating
the flow of air through apparatus 80. As described in detail above
with specific reference to FIG. 1, fans 24 may also be controlled
in conjunction with infrared heaters 14 by controller 28. As shown
in FIG. 3, UHMWPE bars 84 enter apparatus 80, they travel in a
U-shaped pattern between inner wall 85 and outer walls 87. UHMWPE
bars 84 then exit apparatus 80 and continue along conveyor 82 for
additional processing. Additionally, in one exemplary embodiment,
the UHMWPE bars 84 may be placed on conveyor 82 for exposure to
crosslinking radiation prior to UHMWPE bars 84 arriving at
apparatus 80.
[0057] Referring to FIG. 5, an exemplary embodiment of conveyor 82
is shown including connecting portion 54 having elongate shaft 88
with C-shaped hook 90 connected thereto. Connected to UHMWPE bar 84
is attachment member 56 which forms eyelet 92. Eyelet 92 is
configured for receipt on C-shaped hooks 90 of connecting portions
54. Attachment member 56 further includes threaded portion 94
extending in a direction opposite of eyelet 92. Threaded portion 94
allows attachment member 56 to be threaded into UHMWPE bar 84.
While attachment member 56 and connecting portion 54 are described
and depicted herein with specific reference to UHMWPE bars 84 and
apparatus 80, attachment member 56 and connecting portion 54 can be
used with any UHMWPE bars and/or apparatuses described herein.
[0058] As shown in FIG. 5, connecting portion 54, in one exemplary
embodiment, is supported by rotation device 96, which is secured to
conveyor 82. For example, rotation device 96 may support connecting
portion 54 by the securement of connection portion 54 to sprocket
98. In this embodiment, elongate shaft 88 of connecting portion 54
may be welded or otherwise secured to sprocket 98. In one exemplary
embodiment of rotation device 96, motors 100, 102 operate to rotate
sprockets 97, 99, which correspondingly actuate drive chains 101,
103 in opposite directions. As a result of the movement of drive
chains 101, 103, sprocket 98 is rotated to correspondingly rotate
connecting portion 54. Alternatively, motors 100, 102 may be
variable speed motors that are operated at different speeds. In
this embodiment, motors 100, 102 may actuate drive chains 101, 103
in the same direction. Further, in other exemplary embodiments,
sprockets 97, 99 may be different sizes. In another exemplary
embodiment, only a single motor 100, 102 is used. In this
embodiment, one of drive chains 101, 103 may remain stationary
while the other of drive chains 101, 103 is actuated by motor 100,
102.
[0059] As a result of the rotation of connection portion 54,
attachment member 56 and UHMWPE bar 84 are correspondingly rotated.
Thus, operation of rotation device 96 in conjunction with the
operation of conveyor 82 results in rotation device 96 providing
rotational movement of UHMWPE bar 84 while substantially linear
movement of UHMWPE bar 84 is provided by conveyor 82. While
rotation device 96 is described and depicted herein with specific
reference to conveyor 82, rotation device 96 may also be used in
connection with other embodiments of the present invention, such as
center spindle 52 of apparatus 40, shown in FIG. 2 and described in
detail above.
[0060] Advantageously, by utilizing attachment member 56 to secure
UHMWPE bars to corresponding apparatuses for exposing the UHMWPE
bars to infrared radiation, the UHMWPE bars are allowed to expand
as they are subjected to infrared radiation. Specifically, when
exposed to infrared radiation and correspondingly heated, the
UHMWPE bars undergo thermal expansion. If the thermal expansion of
the UHMWPE bars is restricted, the UHMWPE bars may deform from
their intended shape, potentially rendering the resulting melt
annealed bars unusable. By utilizing attachment member 56, UHMWPE
bars 42, 44, 84 are allowed to expand and, when cooled, contract
back to their original shape, without any substantial, permanent
deformation.
[0061] An alternative embodiment of an attachment mechanism for
securing UHMWPE bars to the apparatuses described herein is shown
in FIGS. 6 and 7 as attachment mechanism 100. As shown in FIGS. 6
and 7, attachment mechanism 100 is secured to UHMWPE bar 84.
Specifically, attachment mechanism 100 includes angle braces 102
defining right angles between opposing sides thereof for the
receipt of opposing corners of UHMWPE bar 84. As shown in FIG. 6,
crossbars 104 are received through apertures (shown in dashed
lines) formed in the upper and lower ends of angle braces 102.
Crossbars 104 have a length substantially greater than distance D
extending between opposing corners of UHMWPE bar 84.
[0062] Thus, threaded ends 114 of crossbars 104 are inserted
through upper and lower apertures in opposing angle braces 102
until heads 106 of crossbars 104 contact a first one of angle
braces 102. Springs 108 are then advanced over opposing, threaded
ends 114 of crossbars 104 and positioned thereon. Springs 108 are
secured in position on crossbars 104 by washers 110 and nuts 112.
Specifically, washers 110 are first positioned on crossbars 104 and
then nuts 112 are threadingly engaged with threaded ends 114 of
crossbars 104. Nuts 112 may be tightened until springs 108 are
slightly compressed between nuts 112 and angle braces 102.
Additionally, in one exemplary embodiment, one of crossbars 104
includes an eyelet (not shown) substantially similar to eyelet 92
of attachment member 56. By utilizing an eyelet, attachment
mechanism 100 may be connected to connecting portion 54, shown in
FIG. 5, in a similar manner as described in detail above with
respect to FIG. 5.
[0063] Advantageously, by utilizing attachment mechanism 100 to
secure UHMWPE bars to corresponding apparatuses for exposing the
UHMWPE bars to infrared radiation, the UHMWPE bars are allowed to
expand as they are subjected to the infrared radiation. As
described in detail above with respect to attachment member 56,
UHMWPE bars undergo thermal expansion when heated. Thus, when a
UHMWPE bar secured by attachment mechanism 100 begins to expand,
the UHMWPE bar forces angle braces 102 against the bias of springs
108, thereby compressing springs 108 against washers 110, which are
held in position by nuts 112. By compressing springs 108, the
UHMWPE bars may expand while remaining in substantially the same
position.
[0064] Referring to FIG. 8, another exemplary apparatus for
exposing UHMWPE bars to infrared radiation is depicted as apparatus
120. As shown schematically in FIG. 8, apparatus 120 includes
attachment mechanism 122, shown in more detail in FIG. 9, which
secures UHMWPE bar 84 in position. Positioned adjacent opposing
corners of UHMWPE bar 84 are fans 24. In one exemplary embodiment,
fans 24 are squirrel-cage fans. Additionally, positioned
substantially adjacent each of the opposing sides of UHMWPE bar 84
are infrared heaters 14. To facilitate the reflection of infrared
radiation and to encourage the absorption of the same by UHMWPE bar
84, reflectors 124 may be positioned about apparatus 120 in a
similar manner as described in detail above with reference to
apparatus 10, for example. In one exemplary embodiment, reflectors
124 are arranged to direct the infrared radiation substantially
toward the planer surfaces of UHMWPE bar 84. Additionally, as
discussed in detail above with specific reference to FIG. 1 and
apparatus 10, controller 28 may be utilized to control the
operation of fans 24 and infrared heaters 14.
[0065] Referring to FIG. 9, attachment mechanism 122 facilitates
the insertion and removal of UHMWPE bar 84 from apparatus 120.
Specifically, UHMWPE bar 84 is positioned on carrier 126, having
arms 128 extending from support 130 at a right angle to one another
to form a substantially Y-shaped holder. Apertures 132 extend
through arms 128 and are configured to receive pins 134
therethrough. Thus, by positioning a corner of UHMWPE bar 84
adjacent support 130 such that arms 128 extend along opposing sides
of UHMWPE bar 84, pins 134 may be inserted through apertures 132 in
arms 128 and through UHMWPE bar 84 to secure UHMWPE bar 84 to
carrier 126. In one exemplary embodiment, UHMWPE bar 84 is drilled
to form apertures 140 therein. Pins 134 may then be received
through apertures 132 in arms 128 and apertures 140 in UHMWPE bar
84 to facilitate securement of UHMWPE bar 84 thereto. With UHMWPE
bar 84 in this position, as shown in FIG. 8, UHMWPE bar 84 is
substantially secured within apparatus 120.
[0066] Additionally, as shown in FIG. 9, to facilitate the removal
of carrier 126 and UHMWPE bar 84 from apparatus 120, carrier 126 is
positioned atop bearings 136 which are retained within channel 137
formed in base 138. Referring to FIG. 8, base 138 is secured within
apparatus 120 and, in this position, allows for carrier 126 and
UHMWPE bar 84 to be slid atop bearings 136 in channel 137. By
sliding carrier 126 into and out of apparatus 120, UHMWPE bar 84
may be more readily accessed for attachment to and removal from
carrier 126. In another exemplary embodiment, bearings 136 are
replaced by a chain drive that can be indexed to allow for
substantially automated movement of carrier 126 into and out of
apparatus 120. In another exemplary embodiment, a hydraulic
cylinder may be utilized to move carrier 126 into and out of
apparatus 120.
[0067] Referring to FIG. 10, another exemplary apparatus for
exposing UHMWPE bars to infrared radiation is depicted as apparatus
142. As shown schematically in FIG. 10, apparatus 142 is a larger
version of apparatus 120 shown in FIGS. 8 and 9. For example,
apparatus 142 includes infrared heaters 14 positioned throughout
apparatus 142. Infrared heaters are surrounded by reflective
shielding 144 that directs the infrared radiation toward the planar
surfaces of UHMWPE bars 84 positioned therein. As shown
schematically in FIG. 10, UHMWPE bars 84 are positioned upon
attachment mechanisms 122, described in detail above, and secured
at various heights throughout apparatus 142. Several infrared
heaters 14 are positioned in the center of apparatus 142 and
provide infrared radiation to the planar surfaces of several
different UHMWPE bars 84. Additionally, positioned between UHMWPE
bars 84 is additional reflective shielding 146. In the same manner
as reflective shielding 144, reflective shielding 146 directs
infrared radiation toward UHMWPE bars 84. In one exemplary
embodiment, reflective shielding 146 has a substantially diamond
shaped configuration in cross-section. Additionally, reflective
shielding 146 may also direct cooling air to and exhaust air from
the corners of UHMWPE bars 84 to help to decrease the air
temperature at the surfaces of UHMWPE bars 84. In this manner,
openings (not shown) may be provided within reflective shielding
146. Further, reflective shielding 148 may define a conduit that is
connected to fans 24 (FIG. 1) or other devices that facilitate the
movement of air through apparatus 142.
[0068] Referring to FIGS. 11 and 12, another exemplary apparatus
for exposing UHMWPE bars 84 to infrared radiation is shown as
apparatus 152. Apparatus 152 includes conveyor 150 on which UHMWPE
bars 84 are positioned. Thus, as conveyor 150 is advanced in the
direction of arrows A of FIG. 12, UHMWPE bars 84 travel through
oven 154 having a plurality of infrared heaters 14 positioned
therein. As the UHMWPE bars travel through oven 154, they are
exposed to sufficient infrared radiation to melt anneal UHMWPE bars
84. Additionally, oven 154 may include at least one fan 24 which,
in conjunction with heaters 14, may be operated by controller 28,
as described in detail above with reference to apparatus 10 of FIG.
1. Once UHMWPE bars 84 exit oven 154 on conveyor 150, UHMWPE bars
84 may continue to additional process stations or may be removed
from conveyor 150 for packaging and/or processing.
[0069] Referring to FIGS. 15-17, another exemplary apparatus for
exposing UHMWPE bar 84 to infrared radiation is shown as apparatus
or containment device 156. Containment device 156 includes
container 158 into which UHMWPE bar 84 is positioned. End plates
160, 162 are positioned in sealing engagement with container 158 to
secure UHMWPE bar 84 therein. With UHMWPE bar 84 positioned within
container 158 and containment device 156 sealed, as described in
detail below, container 158 may be flooded with an inert gas, to
purge any oxygen, such as the oxygen component in air, contained
within container 158. By removing oxygen from container 158,
oxidation of UHMWPE bar 84 during infrared melt annealing is
substantially lessened.
[0070] Additionally, in one exemplary embodiment, container 158 is
formed from a material that allows shorter wavelength infrared
radiation to pass therethrough, while blocking longer wavelength
infrared radiation. In one exemplary embodiment, container 158 is
formed of glass. For example, borosilicate glass, such as
Pyrex.RTM. 7740 borosilicate glass commercially available from
Corning, Inc., may be used. Pyrex.RTM. is a registered trademark of
Coming Incorporated of Corning, N.Y. Borosilicate glass has the
ability to withstand thermal shock and also allows for transmission
of approximately ninety percent of near infrared wavelengths, i.e.,
wavelengths shorter than 2.2 .mu.m, therethrough, while blocking
the majority of infrared wavelengths that exceed 2.2 .mu.m, as
shown in FIG. 20. Advantageously, it has been found that shorter
infrared wavelengths, such as in the near infrared region of the
electromagnetic spectrum between visible light and 2.2 .mu.m,
penetrate more deeply into UHMWPE than longer infrared wavelengths
that exceed 2.2 .mu.m. As a result, the longer wavelengths, i.e.,
those over 2.2 .mu.m, are absorbed near the surface of the UHMWPE
causing the thermal energy to be transferred deeper into the UHMWPE
by conduction. By using shorter wavelengths, i.e., those under 2.2
.mu.m, the thermal energy is initial distributed deeper into a
larger volume of the UHMWPE, lessening the need to transfer thermal
energy deeper into the UHMWPE by conduction. This allows for the
transfer of more thermal energy directly into deeper depths of the
material without overheating and/or degrading the UHMWPE at its
surface.
[0071] In order to assemble containment device 156, bar supports
164 are positioned within container 158. Bar supports 164 have a
semi-circular cross-section that provides a flat upper surface for
support of UHMWPE bar 84 and a curved lower surface having a radius
of curvature corresponding to the radius of curvature of container
158. Thus, by positioning bar supports 164 within container 158,
UHMWPE bar 84 may be suspended within container 158 to provide a
separation between portions of UHMWPE bar 84 and container 158.
Once in this position, end plates 160, 162 may be positioned
against adjacent ends of container 158. In order to form an
air-tight seal with container 158, gaskets 166 are positioned
between end plates 160, 162 and container 158. Further, end plates
160, 162 have a plurality of apertures 168 extending therethrough.
Apertures 168 are sized to receive connecting rods 170.
[0072] Connecting rods 170 have opposing threaded ends 172 and are
sized such that threaded ends 172 may extend beyond end plates 160,
162 when connecting rods 170 are passed through apertures 168. In
order to secure connecting rods 170 in position and seal end plates
160, 162 against opposing ends of container 158, nuts 174 are
threadingly engaged with opposing threaded ends 172 of connecting
rods 170. Nuts 174 have internal threads 176 that are configured to
threadingly engage opposing threaded ends 172 of connecting rods
170. By tightening nuts 174 on opposing threaded ends 172 of
connecting rods 170, end plates 160, 162 are pressed against
opposing ends of container 158 with gaskets 166 positioned
therebetween to create an air-tight seal. Additionally, in other
exemplary embodiments, container 158 may have a closed end. Thus,
end plate 162 may be formed as an integral component of container
158. Alternatively, container 158 and end plate 162 may be formed
from a single piece of material to form a monolithic container and
end plate combination.
[0073] Referring to end plate 160, end plate 160 further includes
fluid outlet 178 and fluid inlet 180 that extend through end plate
160 in the form of passageways. Tubing 182 connects to fluid outlet
178 and tubing 184 connects the fluid inlet 180. Fluid inlet 180 is
connected to a source of inert gas, such as nitrogen, which may be
used to purge container 158 of oxygen. Specifically, as the inert
gas enters container 158 through fluid inlet 180, gasses that are
contained within containment device 156 are pushed out through
fluid outlet 178 and tubing 182. In this manner, any gasses, such
as oxygen, that were contained within containment device 158 are
purged therefrom. Additionally, in order to ensure that a
sufficient purging of oxygen has been performed, additional
quantities of inert gas may be released into container 158 through
fluid inlet 180.
[0074] Referring to FIG. 17, containment device 156 is shown
positioned between opposing infrared heaters 14, described in
detail above. As indicated above, infrared heaters 14 may be
activated to generate infrared radiation that is received by UHMWPE
bar 84. Additionally, as infrared radiation passes through
container 158, a portion of the infrared radiation is blocked by
container 158. As a result, only certain wavelengths of infrared
radiation are allowed to pass through container 158 and contact
UHMWPE bar 84. For example, by selecting a material for container
158 that blocks any and/or all of the longer wavelength infrared
radiation, i.e., wavelengths over 2.2 .mu.m, scorching of UHMWPE
bar 84 may be substantially entirely prevented. Additionally,
container 158 may be utilized to hold heated inert gas adjacent
UHMWPE bar 84 and further increase the rate of heating.
Alternatively, additional inert gas may be received within
container 158 and the warm inert gas purged therefrom in a similar
manner as the purging of unwanted gasses described in detail
above.
[0075] By utilizing container 158 in conjunction with the infrared
melt annealing of UHMWPE bar 84 in an inert atmosphere, the
resulting infrared melt annealed UHMWPE bar 84 may be better able
to withstand high temperatures after melt annealing. For example,
UHMWPE bar 84 may be able to be heated to a higher temperature
without detrimental effects on the material properties and/or
overall shape of UHMWPE bar 84. Because of the lack of oxygen in an
inert environment, UHMWPE bar 84 may be processed at a higher
temperature, e.g., between the range of 150.degree. C. to
200.degree. C., without causing oxidation of the surface of UHMWPE
bar 84 as would be the case in an air environment.
[0076] Referring to FIG. 18, a plurality of containment devices 156
are shown in a daisy-chain configuration. Specifically, in this
embodiment, fluid inlet 180 of the first containment device 156 in
the daisy-chain is connected by tubing 186 to a source of inert
gas. Additionally, each fluid outlet 178 of each containment device
156 in the daisy-chain is connected to a corresponding fluid inlet
180 of an adjacent containment device 156. Then, the fluid outlet
178 of the last containment device 156 in the daisy-chain
configuration is connected by tubing 188 to a device configured for
the receipt of the contents of containment devices 158 or is in
fluid communication with the ambient environment, for example. With
the containment devices 156 connected as described in detail above,
inert gas flowing through tubing 186 and entering the first
containment device 156 in the daisy-chain configuration passes
through the first containment device 156 and exits fluid outlet 178
and travels to fluid inlet 180 of an adjacent containment device
156. This process is repeated until the inert gas reaches fluid
outlet 178 of the last containment device 156 in the daisy-chain
configuration. By flooding containment devices 156 with inert gas,
other, unwanted gasses, such as oxygen, contained within
containment devices 156 are forced out of containment devices 156
along the same path that the inert gas travels through the
daisy-chained containment devices 156. In one exemplary embodiment,
additional purging of containment devices 156 may be performed to
ensure that substantially all of the oxygen within containment
devices 156 is successfully evacuated.
[0077] Advantageously, by connecting a plurality of containment
devices 156 together in a daisy-chain configuration, the plurality
of containment devices 156 may be exposed to infrared radiation for
infrared melt annealing substantially simultaneously.
Alternatively, the plurality of containment devices 156 may be
advanced along a conveyor and through an infrared oven in a similar
manner as described in detail above. Additionally, by utilizing the
daisy-chain configuration shown in FIG. 18, inert gas may continue
to be passed through containment device 156 even after
substantially all of the unwanted gasses, such as oxygen, are
removed. As a result, excess heat may be carried away by inert gas
as it passes through the plurality of containment devices 156,
decreasing the temperature of the inert gas surrounding UHMWPE bars
84. Thus, the continued flow of inert gas through containment
devices 156 acts to carry away excess heat in a substantially
similar manner as fans 24, described in detail above. By adjusting
the flow of inert gas through containment devices 156, the
temperature of the inert gas in containment devices 156 may be
maintained at a substantially constant level. Further, the flow of
inert gas may be controlled by a controller, such as controller 28
described in detail above. In addition to carrying away excess
heat, additional purging of containment devices 156 with inert gas
may also remove hydrogen that could evolve from UHMWPE bars 84
during infrared melt annealing.
[0078] Referring to FIG. 19, another exemplary apparatus for
exposing UHMWPE bars 84 to infrared radiation is shown as apparatus
or containment device 190. Containment device 190 may be formed of
nylon, which, in a substantially similar manner as containment
device 156, allows shorter wavelength infrared radiation to pass
therethrough, while blocking any and/or all of the longer
wavelength infrared radiation. In one exemplary embodiment,
containment device 190 is formed as nylon bag 192, which is
constructed from nylon film. Advantageously, the use of a nylon
film, such as a nylon film having a thickness of approximately 25
.mu.m, allows for the creation of a flexible containment device
that has the ability to withstand temperatures in excess of those
required to melt UHMWPE. In one exemplary embodiments, the nylon
film is a 1 millimeter (0.001 ''), 2 millimeter (0.002''), or 5
millimeter (0.005'') thick nylon film commercially available from
KNF Flexpak Corporation of Tamaqua, Pa. In addition, the nylon film
has the ability to transmit greater than ninety-five percent of
near infrared wavelengths shorter than 2.8 .mu.m, while blocking at
least a portion of the infrared wavelengths longer than 2.8 .mu.m,
as shown in FIG. 21 with respect to nylon 6 or polycaprolactam.
Further, a nylon film having a thickness of approximately 25 .mu.m
is also less permeable to oxygen than polyethylene film having a
similar thickness. Specifically, a nylon film having a 25 .mu.m
thickness has an oxygen permeability of 2.5
(ml/m.sup.2/MPa/Day).sup.2, while a polyethylene film having a
thickness of approximately 25 .mu.m has an oxygen permeability of
71 (ml/m.sup.2/MPa/Day).sup.2.
[0079] As shown in FIG. 19, UHMWPE bar 84 is positioned within
containment device 190. Containment device 190 is then sealed to
prevent any gasses from entering or exiting containment device 190.
Prior to sealing containment device 190, containment device 190 may
be purged with an inert gas to remove air and/or oxygen therefrom.
Additionally, in one exemplary embodiment, containment device 190
is vacuum sealed, such that containment device 190 lies
substantially adjacent UHMWPE bar 84 with substantially no air
and/or oxygen therebetween. In order to expose containment device
190 and UHMWPE bar 84 to infrared irradiation, UHMWPE bar 84 and,
correspondingly, containment device 190 are positioned on supports
194 extending between infrared heaters 14.
[0080] In other exemplary embodiment, in order to process a
plurality of UHMWPE bars without the need to utilize a
corresponding plurality of containment devices 156, 190, an oven
modified for use in infrared melt annealing, such as oven 154
described in detail above, may be further modified to include a
sheet of material positioned between UHMWPE bars 84 and infrared
heaters 14. By selecting a material that blocks any and/or all of
the longer wavelength infrared radiation, while allowing shorter
wavelength infrared radiation to pass therethrough, the material
may act in a substantially similar manner as the material forming
containers 158, described above. In one exemplary embodiment, the
material positioned between UHMWPE bars 84 and the infrared heaters
is glass. In another exemplary embodiment, the material positioned
between UHMWPE bars 84 and the infrared heaters is nylon.
[0081] Further, in order to remove the air and/or oxygen from the
oven and to create an inert environment, the oven may be a vacuum
oven, for example. By subjecting the oven to a vacuum and then
backfilling the oven with an inert gas, such as nitrogen, an inert
environment may be created. Alternatively, in another exemplary
embodiment, an inert environment may be created in the oven, but no
material is positioned between UHMWPE bars 84 and the infrared
heaters to block the passage of longer wavelength infrared
radiation, while allowing shorter wavelength infrared radiation to
pass therethrough. Thus, in this embodiment, infrared melt
annealing is performed in the inert environment created in the oven
and UHMWPE bars 84 received substantially all of the wavelengths of
infrared irradiation generated by the infrared heaters in the
oven.
EXAMPLES
[0082] The following non-limiting Examples illustrate various
features and characteristics of the present invention, which is not
to be construed as limited thereto. The following abbreviations are
used throughout the Examples unless otherwise indicated.
TABLE-US-00001 TABLE 1 Abbreviations Abbreviation Full Word kGy
kilo Gray min minute .degree. degrees C. Celsius FTIR Fourier
Transform Infrared Spectroscopy UTS ultimate tensile strength
UHMWPE ultrahigh molecular weight polyethylene '' inches OI
Oxidation Index DSC Differential Scanning Calorimetry TVI
trans-vinylene index cm centimeter DMA dynamic mechanical analyzer
Hz hertz P net radiated power A radiating area .sigma. Stefan's
constant e emissivity (=1 for an ideal radiator) T temperature of
emitter T.sub.C temperature of material c speed of light .lamda.
wavelength e base of natural log h Planck constant k Boltzman
constant E illuminance I pointance ND not detectable .mu.m
micrometer .pi. 3.14159265 r distance K kelvin VF.sub.(1-2) view
factor
Example 1
[0083] Watt Densities of Thermal Radiation Generated by Different
Emitters
[0084] Calculations were performed to identify the increased watt
density that is generated by using thermal radiation. Specifically,
as set forth in TABLE 2 below, the watt density emitted from both
the stainless steel walls of a convection oven and a tungsten aged
filament from an infrared heater were calculated. The watt density,
P, expressed as watts per square centimeter, was calculated using
the Stefan-Boltzmann Law, i.e., P=e.sigma.A(T.sup.4-T.sub.C.sup.4)
, where .sigma. is equal to 5.6703.times.10.sup.-8
watt/m.sup.2K.sup.4. In performing each of the calculations, a
radiating area, A, of one square centimeter was used.
[0085] Additionally, the watt density received, i.e., the amount of
radiation that reaches a material to be heated, was calculated for
different distances between the radiation source and the material
to be heated. Specifically, the watt density received at 1 inch,
i.e., when 1 inch separates the source of the radiation and the
material to be heated, and at 6 inches, i.e., when 6 inches
separate the source of the radiation and the material to be heated,
were determined by calculating the heat flow at a given distance
from the radiation source and multiplying the same by the
emissivity coefficient of the material, which is set forth in TABLE
2 below. The heat flow may be calculated using the following
equation:
q=56.69.times.10.sup.-9.times.VF.sub.(1-2).times.A.times.(T.sup.A-T.sub.-
C.sup.2),
where q is the heat flow, A is the area of the opposing flat
surfaces, Tis the temperature of the radiation emitter, and T.sub.C
is the temperature of the material or part to be heated.
Additionally, VF.sub.(1-2) is the view factor, which at 1 inch is
equal to 0.0448244 and at 6 inches is equal to 0.0013666. An area,
A, of 1 square centimeter was used in performing each of the
calculations.
TABLE-US-00002 TABLE 2 Watts/cm.sup.2 Watts/cm.sup.2 Emissivity
Emitter Part Watts/cm.sup.2 received at received at 6 Emitter
Coefficient Temp. Temp. Emitted 1 inch inches Stainless 0.075 to
0.85 423 K 296 K 0.010 to 0.117 4.64E-04 to 1.42E-05 to Steel
5.26E-03 1.60E-04 Tungsten 0.032 to 0.35 2,477 K 296 K 6.83 to
74.71 0.31 to 0.009 to filament 3.35 0.102
Example 2
[0086] Feasibility of Utilizing Infrared Radiation to Melt Anneal
Crosslinked UHMWPE
[0087] The feasibility of utilizing infrared radiation to melt
anneal crosslinked UHMWPE and the mechanical properties of the
resulting infrared melt annealed UHMWPE were investigated. To
perform this investigation, Design Expert 6.0.10 software, obtained
from Stat-Ease, Inc. Minneapolis, Minn., was utilized to create a
Design of Experiment (DOE) to evaluate the mechanical properties of
the infrared melt annealed crosslinked UHMWPE. The DOE evaluated
three different variables: the maximum temperature of the UHMWPE,
cooling of the external surface of the UHMWPE, and the amount of
time elapsed during temperature ramp up.
[0088] Medical grade UHMWPE powder, GUR 1050, was obtained from
Ticona, having North American headquarters in Florence, Ky. The
UHMWPE was compression molded into approximately 3.5 '' square
bars. The bar was then cut into sections measuring 6'' in length.
Each 6'' section was then subjected to electron beam irradiation in
air and received a 100 kGy dose. Once irradiated, each 6'' section
of UHMWPE bar was immediately packaged in nitrogen where it
remained until the time of testing.
[0089] In order to subject the sections of UHMWPE bar to infrared
radiation, two Chromalox.RTM. T-3 quartz heaters were obtained from
Thermtech Systems, Inc. of Chesterfield, Ind. The heaters were
positioned 6'' from where a face of a section of the UHMWPE bar is
positioned during exposure to the infrared radiation, as shown in
FIG. 13. Referring to FIG. 13, an exemplary section of UHMWPE bar
200 and an exemplary infrared heater 202 are shown. Once positioned
adjacent the heaters, the section of UHMWPE bar was received on a
rotatable bar 204 and rotated using a small motor. The sections
were then heated by infrared radiation to a maximum temperature
selected from 140.degree. C. and 150.degree. C. and some of the
sections were ramped to reach the maximum temperature in four
hours, which is identified in TABLE 3 with a "y" in the ramp
column. During the heating of some of the sections, as identified
in TABLE 3 below, a fan was activated to facilitate cooling of the
outer surface of the section of the UHMWPE bar.
[0090] A portion of each bar was then microtomed into 2000 micron
thick films. These films were then subjected to FTIR analysis on a
Bruker Optics FTIR spectrometer, available from Bruker Optics of
Billerica, Mass. The FTIR results were analyzed to determine the OI
and the TVI. The OI was determined by calculating the ratio of the
area under the carbonyl peak on the FTIR chart at 1765-1680
cm.sup.-1 to the area of the polyethylene peak at 1392-1330
cm.sup.-1. The TVI was determined by calculating the ratio of the
area on the FTIR chart under the vinyl peak at 980-947 cm.sup.-1 to
the area under the polyethylene peak at 1392-1330 cm.sup.-1.
[0091] Additional testing was then performed to determine the izod
impact strength, elongation, UTS, YS, storage modulus, percentage
crystallinity, and free radical concentration. The mechanical
properties were tested according to corresponding available ASTM
standards for UHMWPE. Specifically, Type V tensile specimens, as
defined by the American Society for Testing and Materials (ASTM)
Standard D638, Standard Test Method for Tensile Properties of
Plastics, were machined and subjected to elongation, UTS, and YS
testing in accordance with ASTM Standard D638. Izod specimens were
also machined and subjected to testing according to ASTM Standard
F-648, Standard Test Methods for Ultra-High-Molecular-Weight
Polyethylene Power and Fabricated Form for Surgical Implants. The %
crystallinity was determined using DSC and measuring the
crystallinity between 40.degree. C. and 160.degree. C.
Additionally, the storage modulus was measured using a DMA. This
method begins by ramping the temperature from room temperature to
150.degree. C. at a rate of 10.degree. C./min and then ramping the
temperature from 150.degree. C. to 210.degree. C. at a rate of
2.degree. C./min at 1 Hz. The DMA measurement corresponds to the
Storage Modulus of the UHMWPE at 200.degree. C. Additionally, the
free radical concentration of the UHMWPE was analyzed using a
Bruker EMX/EPR (electron paramagnetic resonance) spectrometer,
which has a detection limit of 0.01.times.10.sup.15 spins/gram and
is available from Bruker Optics of Billerica, Mass.
[0092] Based on the results of the analysis, the infrared melt
annealed crosslinked UHMWPE had OI values lower than the control,
which in this case is a convection oven melt annealed crosslinked
UHMWPE, and had substantially similar or improved mechanical
properties under all of the varying test conditions.
TABLE-US-00003 TABLE 3 Mechanical Properties of Infrared Melt
Annealed Crosslinked UHMWPE Oxidation Index at Run Temp (deg C.)
Fan Ramp Material 2000 microns Control -- -- 1050 0.0900 1 140 y n
1050 0.0234 2 140 n n 1050 0.0087 3 140 y y 1050 0.0073 4 140 n y
1050 0.0289 5 150 y y 1050 0.0162 6 150 n y 1050 0.0052 7 150 y n
1050 0.0007 8 150 n n 1050 0.0056 Elongation Izod DMA ESR Run %
(kJ/m{circumflex over ( )}2) (MPa @ 200 C.) (10{circumflex over (
)}15 spins/gram) Control 231 57 7.605 0.09 1 271 Not tested 7.696
0.04 2 271 69.9 7.586 0.06 3 279 66.9 7.433 0.02 4 280 65.3 7.524
0.04 5 277 66.0 7.327 0.04 6 261 70.3 7.428 0.05 7 259 71.3 7.659
0.08 8 278 71.6 7.136 0.05
Example 3
[0093] Effects of Varying the Distance of the Infrared Source from
the UHMWPE
[0094] The optimal distance between an infrared heating element and
crosslinked UHMWPE for infrared melt annealing was investigated. To
perform this investigation, Design Expert 6.0.10 software, obtained
from Stat-Ease, Inc. Minneapolis, Minn., was utilized to create a
Design of Experiment (DOE) to evaluate the mechanical properties of
the infrared melt annealed crosslinked UHMWPE. The DOE evaluated
two different variables: the distance from an infrared heating
element to a face of the UHMWPE and the percentage of total heating
time that a fan was activated to cool the surface of the bar.
[0095] Medical grade UHMWPE powder, GUR 1050, was obtained from
Ticona, having North American headquarters in Florence, Ky. The
UHMWPE was compression molded into approximately 3.5'' square bars.
The bar was then cut into sections measuring 6'' in length. Each
6'' section was then subjected to electron beam irradiation and
received a 100 kGy dose. Once irradiated, each 6'' section of
UHMWPE bar was immediately packaged in nitrogen where it remained
until the time of testing.
[0096] In order to subject the sections of UHMWPE bar to infrared
radiation, four Chromalox.RTM. T-3 quartz heaters were obtained
from Thermtech Systems, Inc. of Chesterfield, Ind. The heaters were
positioned in the four corners of a square-shaped steel frame. The
sections of UHMWPE bar were then removed from their packaging and
positioned in a holder that held the sections stationary between
the four heaters so that the flat sides of the sections were each
directly facing one of the infrared heaters, as shown in FIG. 14.
Referring to FIG. 14, an exemplary section of UHMWPE bar 206 and
exemplary infrared heaters 208 are shown. The sections were
positioned in the frame at a distance from the infrared heaters
selected from 5 inches, 7 inches, and 10 inches. Additionally,
during the heating of the sections, as identified in TABLE 4 below,
a fan was activated to facilitate cooling of the outer surface of
the section of the UHMWPE bar for a time selected from 0, 50, and
100 percent of the total heating time. The UHMWPE sections were
then allowed to cool.
[0097] Testing was then performed to determine the izod impact
strength, elongation, UTS, YS, and free radical concentration. The
mechanical properties were tested according to ASTM standards
corresponding to UHMWPE. Specifically, Type V tensile specimens, as
defined by the American Society for Testing and Materials (ASTM)
Standard D638, Standard Test Method for Tensile Properties of
Plastics, were machined and subjected to elongation, UTS, and YS
testing in accordance with ASTM Standard D638. Izod specimens were
also machined and subjected to testing according to ASTM Standard
F-648, Ultra-High-Molecular-Weight Polyethylene Powder and
Fabricated Form for Surgical Implants. Additionally, the free
radical concentration was analyzed using a Bruker EMX/EPR (electron
paramagnetic resonance) spectrometer, which has a detection limit
of 0.01.times.10.sup.15 spins/gram and is available from Bruker
Optics of Billerica, Mass.
[0098] Overall, the experiment showed that the UHMWPE had
substantially equivalent or better mechanical properties
irrespective of heater distance up to 10 inches.
TABLE-US-00004 TABLE 4 Effects of Radiation Distance on the
Material Properties of Infrared Melt Annealed Crosslinked UHMWPE
Heater Distatnce ESR From Bar % of Time UTS YS Izod (10{circumflex
over ( )}15 Sample (Inches) Fan Is On Elongation % (MPa) (MPa)
(kJ/m{circumflex over ( )}2) spins/gram) Control -- -- 231 39.4
21.03 57 0.09 7 4 0 232 34.0 20.61 63.9 Non Detectable 1 4 50 245
33.4 20.78 60.3 Non Detectable 11 4 50 224 32.8 20.67 56.2 Non
Detectable 6 4 100 348 39.7 20.57 78.1 Non Detectable 4 7 0 228
32.7 20.68 59.9 Non Detectable 9 7 0 316 36.9 20.24 78.0 Non
Detectable 10 7 50 335 39.1 20.28 79.0 Non Detectable 13 7 50 324
36.4 20.48 78.3 Non Detectable 3 7 100 301 38.0 20.66 80.2 Non
Detectable 12 7 100 230 33.8 20.38 57.5 Non Detectable 5 10 0 216
35.7 20.25 58.1 Non Detectable 8 10 50 225 33.0 20.49 56.1 Non
Detectable 14 10 50 241 34.2 20.46 58.6 Non Detectable 2 10 100 223
32.9 20.45 59.3 2.84
Example 4
[0099] Effects of Different Wavelengths of Infrared Radiation
[0100] The effects of using different wavelengths of infrared
radiation to infrared melt anneal crosslinked UHMWPE was
investigated. Medical grade UHMWPE powder, GUR 1050, was obtained
from Ticona, having North American headquarters in Florence, Ky.
The UHMWPE was compression molded into approximately 3.5'' square
bars. The bar was then cut into sections measuring 6'' in length.
Each 6'' section was then subjected to electron beam irradiation
and received a 100 kGy dose. Once irradiated, each 6'' section of
UHMWPE bar was immediately packaged in nitrogen where it remained
until the time of testing.
[0101] Three different types of infrared heaters were acquired, as
set forth in TABLE 5 below. In order to expose the UHMWPE sections
to infrared radiation, two heaters of the same type were positioned
approximately 24 inches apart from and facing one another. The
heaters were attached to a steel frame and held stationary. The
sections of the UHMWPE bar were mounted between the heaters so that
the flat sides of the bar were facing the heaters. A thermocouple
was mounted inside the sections of the UHMWPE bar to monitor the
temperature within the UHMWPE bar. The bar was heated to
150.degree. C. and the time that elapsed until the bar was
substantially entirely melted, i.e., the time that elapsed from the
initiation of the heating until the opaque crystalline regions of
the bar became amorphous and, thus, were optically transparent as
determined by visual observation, was recorded. This process was
repeated for each type of heater set forth in TABLE 5 below.
TABLE-US-00005 TABLE 5 Types of Infrared Heaters Utilized
Manufacturer Type of Heater Manufacturer Identification Wavelength
Radiant Watlow Flat Panel 24'' Long (8-15 St. Louis, MO 2,880
watts/240 V micrometers) Quartz Ramax 1515 25.5'' Medium (3-8 1,250
watts/240 V micrometers) Tungsten QR16B230 16'' Short (1.4-3 1,600
watts/240 V micrometers)
[0102] Once all of the sections of the UHMWPE bar had been tested,
the material properties of the resulting sections were analyzed. A
portion of each section was microtomed into 2000 micron thick
films. These films were then subjected to FTIR analysis on a Bruker
Optics FTIR spectrometer, available from Bruker Optics of
Billerica, Mass. The FTIR results were analyzed to determine the
OI. The OI was determined by calculating the ratio of the area
under the carbonyl peak on the FTIR chart at 1765-1680 cm.sup.-1 to
the area of the polyethylene peak at 1392-1330 cm.sup.-1.
[0103] Additional testing was then performed to determine the
elongation, YS, UTS, and free radical concentration. The mechanical
properties were tested according to ASTM standards corresponding to
UHMWPE. Specifically, Type V tensile specimens, as defined by the
American Society for Testing and Materials (ASTM) Standard D638,
Standard Test Method for Tensile Properties of Plastics, were
machined and subjected to elongation, UTS, and YS testing in
accordance with ASTM Standard D638. Additionally, the free radical
concentration was analyzed using a Bruker EMX/EPR (electron
paramagnetic resonance) spectrometer, which has a detection limit
of 0.01.times.10.sup.15 spins/gram and is available from Bruker
Optics of Billerica, Mass.
[0104] The analysis, the results of which are set forth below in
TABLE 6, showed that the material properties did not vary
substantially between wavelengths. However, the polyethylene
appeared most quickly to absorb the short wavelengths, i.e., those
generated by the heaters with tungsten filaments.
TABLE-US-00006 TABLE 6 Effects of Radiation Wavelength on the
Mechanical Properties of Infrared Irradiated Crosslinked UHMWPE
Oxidation ESR Index at 2000 UTS YS (10{circumflex over ( )}15 Time
to Melt (Hours) microns Elongation % (MPa) (MPa) spins/gram) (3.6
.times. 3.6 .times. 6'' bar) Control 0.0900 231.4 39.40 21.03 0.09
8 (convection oven) Radiant 0.0322 277.1 46.89 20.07 ND 3.5 Quartz
0.0340 292.3 46.51 19.44 ND 2 Tungsten 0.0056 278.4 46.12 19.57
0.05 1.25
Example 5
[0105] Effects of Infrared Melt Annealing in an Inert
Atmosphere
[0106] In order to examine the effects of infrared melt annealing
in an inert atmosphere on UHMWPE bar stock, several experiments
were conducted.
Bar Stock Section 1
[0107] Bar stock section 1 was formed from medical grade UHMWPE
powder, GUR 1050, obtained from Ticona, having North American
headquarters in Florence, Ky. The UHMWPE was compression molded
into an approximately 1.9'' square bar. The bar was then cut into a
section measuring 3'' in length. The 3'' section was then subjected
to electron beam irradiation and received a 100 kGy dose. Once
irradiated, the 3'' section of UHMWPE bar was immediately packaged
in nitrogen where it remained until the time of testing.
[0108] Bar stock section 1, which, as indicated above, was in the
form of a 1.9 inch by 1.9 inch by 3 inch rectangular section of
UHMWPE bar, was placed in a quart canning jar that was obtained
from Heinz Foods of Pittsburg, Pa. The canning jar was modified by
providing inlet and outlet passageways in the lid of the jar. The
inlet passageway of the jar was connected to a source of nitrogen,
while the outlet passageway was connected through vacuum tubing to
a bone cement vacuum pump model S/9 No. 9, Lot No. 4234,
manufactured by Scandimed of Glostrop, Denmark, and distributed by
Zimmer, Inc. The canning jar was then positioned between two
opposing 600 watt T3 halogen lamps generating infrared irradiation
having an approximate wavelength of 1.0-1.5 microns. The jar was
then purged three times with nitrogen by supplying nitrogen to the
jar through the inlet, which forced out the gaseous contents of the
jar through the outlet in the lid of the jar. The halogen lamps
where then turned on to full power for the duration of the heating
and a neutral pressure was maintain in the jar during heating. The
jar was purged three times as the bar was heated in order to remove
any hydrogen that may have evolved during the heating.
[0109] After 28 minutes, the bar was visually determined to have
completely melted, as evidenced by a change from opaque to
semi-transparent. The time to melt of 28 minutes is substantially
less than the time required to melt the bar using the same heaters
in the open air. This is believed to be caused by the passage of
only short wavelength infrared irradiation combined with the
insulating and greenhouse type effects of the jar. With the lamps
turned off, the bar was allowed to remain in the jar to cool. The
cooling time for the bar was longer than would have been expected
in the ambient environment and is believed to also have resulted
from the insulating and greenhouse type effects of the jar.
Additionally, upon visual inspection after cooling, the bar had no
discoloration.
Bar Stock Section 2
[0110] Bar stock section 2 was formed from medical grade UHMWPE
powder, GUR 1050, obtained from Ticona, having North American
headquarters in Florence, Ky. The UHMWPE was compression molded
into an approximately 2.13'' square bar. The bar was then cut into
a section measuring 3'' in length. The 3'' section was then
subjected to electron beam irradiation and received a 100 kGy dose.
Once irradiated, the 3'' section of UHMWPE bar was immediately
packaged in nitrogen where it remained until the time of
testing.
[0111] Bar stock section 2, which, as indicated above, was in the
form of a 2.13 inch by 2.13 inch by 3 inch rectangular section of
UHMWPE bar, was placed in a half gallon canning jar that was
obtained from Pinnacle Foods of Allentown, Pa. The canning jar was
modified by providing inlet and outlet passageways in the lid of
the jar. The inlet passageway of the jar was connected to a source
of nitrogen, while the outlet passageway was connected through
vacuum tubing to a bone cement vacuum pump model S/9 No. 9, Lot No.
4234, manufactured by Scandimed of Glostrop, Denmark, and
distributed by Zimmer, Inc. The canning jar was then positioned
between two opposing 600 watt T3 halogen lamps generating infrared
irradiation having an approximate wavelength of 1.0-1.5 microns.
The jar was then purged three times with nitrogen by supplying
nitrogen to the jar through the inlet, which forced out the gaseous
contents of the jar through the outlet. The lamps where then turned
on and a partial vacuum nitrogen pressure was maintained in the jar
during heating. Additionally, the jar was purged three times during
the heating cycle to remove any hydrogen that may have evolved
during the heating.
[0112] After 45 minutes, the bar was visually determined to have
completely melted, as evidenced by a change from opaque to
semi-transparent. The time to melt of 45 minutes is substantially
less than the time required to melt the bar using the same heaters
in the open air. This is believed to be caused by the passage of
only short wavelength infrared irradiation combined with the
insulating and greenhouse type effects of the jar. With the lamps
turned off, the bar was allowed to remain in the jar to cool. The
cooling time for the bar was longer than would have been expected
in the ambient environment and is believed to also have resulted
from the insulating and greenhouse type effects of the jar.
Additionally, upon visual inspection after cooling, the bar had no
discoloration.
[0113] Bar Stock Section 3
[0114] Bar stock section 3 was formed from medical grade UHMWPE
powder, GUR 1050, obtained from Ticona, having North American
headquarters in Florence, Ky. The UHMWPE was compression molded
into an approximately 2.13'' square bar. The bar was then cut into
a section measuring 3'' in length. The 3'' section was then
subjected to electron beam irradiation and received a 100 kGy dose.
Once irradiated, the 3'' section of UHMWPE bar was immediately
packaged in nitrogen where it remained until the time of
testing.
[0115] Bar stock section 3, which, as indicated above, was a 2.13
inch by 2.13 inch by 3 inch rectangular section of UHMWPE bar, was
placed in nylon pouch. The pouch was formed from 0.001'' thick
nylon film cut from a 19'' by 23.5'' Reynolds.RTM. brand oven bag
commercially available from Reynolds Food Packing Group of
Richmond, Va. Reynolds.RTM. is a registered trademark of Reynolds
Metal Corporation of Richmond, Va. The bag was evacuated, purged
with nitrogen, and then heat sealed to create an inert environment
within the bag. The cooking bag containing the UHMWPE bar was then
positioned between two opposing 600 watt T3 halogen lamps
generating infrared irradiation having an approximate wavelength of
1.0-1.5 microns. The lamps where then turned on and the melting of
the UHMWPE bar was visually observed.
[0116] After 30 minutes, the bar was visually determined to have
completely melted, as evidenced by a change from opaque to
semi-transparent. The time to melt of 30 minutes is substantially
less than the time required to melt the bar using the same heaters
in the open air. This is believed to be caused by the passage of
only short wavelength infrared irradiation combined with the
insulating and greenhouse type effects of the cooking bag. The bar
was then allowed to cool and was removed from the cooking bag. Upon
visual inspection after cooling, the bar was discolored in the
areas where it was in direct contact with the cooking bag.
[0117] Bar Stock 4
[0118] Bar stock section 4 was formed from medical grade UHMWPE
powder, GUR 1050, obtained from Ticona, having North American
headquarters in Florence, Ky. The UHMWPE was compression molded
into an approximately 2.2'' square bar. The bar was then cut into a
section measuring 3'' in length. The 3'' section was then subjected
to electron beam irradiation and received a 100 kGy dose. Once
irradiated, the 3'' section of UHMWPE bar was immediately packaged
in nitrogen where it remained until the time of testing.
[0119] Bar stock section 4, which, as indicated above, was in the
form of a 2.2 inch by 2.2 inch by 3 inch rectangular section of
UHMWPE bar, was placed in a quart canning jar that was obtained
from Heinz Foods of Pittsburg, Pa. The canning jar was modified by
providing inlet and outlet passageways in the lid of the jar. The
inlet passageway of the jar was connected to a source of nitrogen,
while the outlet passageway was connected through vacuum tubing to
a bone cement vacuum pump model S/9 No. 9, Lot No. 4234,
manufactured by Scandimed of Glostrop, Denmark, and distributed by
Zimmer, Inc. The canning jar was then positioned between two
opposing 600 watt T3 halogen lamps generating infrared irradiation
having an approximate wavelength of 1.0-1.5 microns. The jar was
then purged three times with nitrogen by supplying nitrogen to the
jar through the inlet, which forced out the gaseous contents of the
jar through the outlet in the lid of the jar. The halogen lamps
where then turned on to full power for the duration of the heating
and a neutral pressure was maintain in the jar during heating. The
jar was purged three times as the bar was heated in order to remove
any hydrogen that may have evolved during the heating.
[0120] After 47 minutes, the bar was visually determined to have
completely melted, as evidenced by a change from being opaque to
being completely optically transparent. Once the bar had cooled, a
portion of the bar was then microtomed into 2000 micron thick
films. These films were then subjected to FTIR analysis on a Bruker
Optics FTIR spectrometer, available from Bruker Optics of
Billerica, Mass. The FTIR results were analyzed to determine the OI
of the films. The OI was determined by calculating the ratio of the
area under the carbonyl peak on the FTIR chart at 1765-1680
cm.sup.-1 to the area of the polyethylene peak at 1392-1330
cm.sup.-1. The results of the testing are shown graphically in FIG.
22. Referring to FIG. 22, the normalized OI for the sample was
0.0097 at a depth of 2,000 microns below the exterior surface of
the bar and was below 0.1000 at the exterior surface of the bar. In
contrast, when a similar bar was infrared melt annealed in air, the
resulting normalized OI for the bar was 0.1263 at a depth of 2,000
microns below the exterior surface of the bar and was over 0.4000
at the exterior surface of the bar, as shown in FIG. 23.
[0121] While this invention has been described as having a
preferred design, the present invention can be further modified
within the spirit and scope of this disclosure. This application is
therefore intended to cover any variations, uses, or adaptations of
the invention using its general principles. Further, this
application is intended to cover such departures from the present
disclosure as come within known or customary practice in the art to
which this invention pertains and which fall within the limits of
the appended claims.
* * * * *